1、BRITISH STANDARD BS ISO 14899:2001 Plastics Polyols for use in the production of polyurethane Determination of basicity ICS 49.025.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 14899:2001 This British Standard, having been prepared under the direction of the Sector
2、Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 May 2001 BSI 05-2001 ISBN 0 580 37395 9 National foreword This British Standard reproduces verbatim ISO 14899:2001 and implements it as the UK national standard. The UK par
3、ticipation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards
4、which implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purpor
5、t to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible internatio
6、nal/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title
7、 page, pages ii to v, a blank page, pages 1 to 5 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsReference number ISO 14899:2001(E) INTERNATIONAL STANDARD ISO 14899 First editio
8、n 2001-02-15 Plast icsPo ly olsfo ru seinth e production of polyurethane Determination of basicity Plastiques Polyols pour la production du polyurthanne Dtermination de la basicitISO 14899:2001(E) f t ii ISO 14899:2001(E)iii Contents Page Foreword.iv Introduction.v 1 Scope 1 2 Normative references 1
9、 3 Terms and definitions .1 4 Principle2 5 Sampling.2 6 Interferences 2 7 Reagents.2 8 Apparatus .2 9 Procedure .3 10 Expression of results 3 11 Precision and bias .4 12 Test report 4 Bibliography5ISO 14899:2001(E) iv Foreword ISO (the International Organization for Standardization) is a worldwide f
10、ederation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that co
11、mmittee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accor
12、dance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention i
13、s drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 14899 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommi
14、ttee SC 12, Thermosetting materials.ISO 14899:2001(E)v Introduction This method is for the determination of trace amounts of basicity in polyether polyols, which are used in the preparation of polyurethane prepolymers and polyurethane products. Knowledge of this value is important to prevent gelatio
15、n during prepolymer production and to control reaction rates during polyurethane preparation. The method, known as the CPR (controlled polymerization rate) analysis, has become an accepted industry practice, a version of which has been published as part of JIS K 1557.INTERNATIONAL STANDARD ISO 14899
16、:2001(E)1 Plastics Polyols for use in the production of polyurethane Determination of basicity WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use.
17、It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies a method for the measurement of trace amounts of basic materials present in polyether polyols used
18、 in the production of polyurethanes. It is important to know the trace amount of basicity in a polyol to prevent gelation of the reaction mass during the production of polyurethane prepolymers. It is also useful to control the basicity in polyols used for polyurethane production to assure consistent
19、 and reproducible reaction behaviour. This method is suitable for quality control, as a specification test and for research. The applicable range is 0 gt o5 0 g/g, expressed as KOH. The method is not applicable to amine-based polyols. The values may be reported as CPR (controlled polymerization rate
20、) units. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties
21、to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain
22、registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test methods. ISO 6353-2:1983, Reagents for chemical analysis Part 2: Specifications First series.
23、ISO 6353-3:1987, Reagents for chemical analysis Part 3: Specifications Second series. 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 polyurethane a polymer prepared by the reaction of an organic di- or polyisocyanate with compo
24、unds containing two or more hydroxyl groupsISO 14899:2001(E) 2 3.2 CPR value controlled polymerization rate value the number of microequivalents of base in a 30 g test portion of polyol (i.e. meq of base in 30 kg of polyol) 4P r i n c i p l e A 30 g test portion of polyol is diluted with methanol an
25、d titrated with aqueous 0,01 mol/l HCl. The results are compared with a blank titration of the methanol. 5 Sampling Draw samples from a well-mixed vessel into a thoroughly cleaned and dry borosilicate glass container (soft glass containers are not acceptable). If sampling from a line or valve, flush
26、 the line thoroughly with the product before starting to draw the sample. Seal the sample until analysis. 6 Interferences Any acidic or basic materials inadvertently introduced into the sample will cause errors in the analysis. Any material capable of serving as a buffer may interfere with the analy
27、sis by obscuring the titration end point. Some samples may contain traces of several different compounds which may have the effect of causing multiple breaks in the titration curve, making interpretation difficult. This analysis is not applicable to amine-based polyols. 7 Reagents Reagent-grade chem
28、icals shall be used in all determinations. Unless otherwise indicated, it is intended that all reagents conform to the specifications of ISO 6353-1, ISO 6353-2 and ISO 6353-3, although other grades may be used provided that it is first determined that the reagent is of sufficiently high purity to pe
29、rmit its use without lessening the accuracy of the determination. Unless otherwise indicated, references to water shall be understood to mean grade 2 reagent water as defined by ISO 3696:1987. 7.1 Hydrochloric acid, standard solution, 0,01 mol/l. Prepare and standardize in accordance with good pract
30、ice, using potassium acid phthalate (7.2) as a primary standard. Standardize to detect changes of 0,000 1 mol/l. 7.2 Potassium acid phthalate. Use a certified primary standard. 7.3 Methanol, reagent grade, conforming to ISO 6353-2. 8 Apparatus 8.1 Autotitrator, capable of determining multiple end po
31、ints, equipped with a pair of electrodes or a combination glass calomel electrode, a 5 ml burette and a recorder. 8.2 Burette, or other automatic dispensing device, capable of dispensing 50 ml 0,1 ml.ISO 14899:2001(E)3 8.3 Balance, capable of weighing 30 g test portions to 1mg . 8.4 Titration flask,
32、 100 ml, or other suitable titration vessel. 8.5 Magnetic stirrer, equipped with an inert stirrer bar, or equivalent. 9 Procedure 9.1 Set up the titrator (8.1) for titrations having a maximum titrant volume of 5 ml. 9.2 Add 50 ml of methanol (7.3) to a 100 ml titration flask (8.4) for use as a solve
33、nt blank. NOTE Some popular automatic titrimeters are equipped with 100 ml titration vessels. With other titrimeters, an acceptable variation of the method is to use 100 ml of methanol in a 150 ml titration vessel, as is done in JIS K 1557. 9.3 Titrate the solvent blank with 0,01 mol/l HCl (7.1) and
34、 record the volume of titrant used. The end point is taken as the point of inflection of the last end point on the titration curve. The blank should consume less than 0,2mlof0,01mol/lHCl. 9.4 Into a 100 ml titration flask, weigh about 30 g of sample to the nearest 1 mg. Add 50 ml of methanol and sti
35、r until well mixed. (See the note to 9.2.) 9.5 Titrate with 0,01 mol/l HCl and record the volume of titrant up to the last end point. NOTE Depending on the sample being analysed, as many as three inflection points may be seen. Use the last end point. 10 Expression of results 10.1 Calculate the CPR v
36、alue using the following equation: CPR value = SB 30 ( ) 1000 VVM m where V S is the volume of HCl needed to titrate the test portion, in ml; V B is the volume of HCl needed to titrate the blank, in ml; M is the molarity of the HCl, in mol/l; m is the mass of the test portion, in g. 10.2 The basicit
37、y may also be calculated as g KOH/g of sample using the following equation: g KOH/g of sample = SB 56,1 ( ) 1000 VVM m ISO 14899:2001(E) 4 11 Precision and bias 11.1 Precision 11.1.1 Use the criteria for repeatability and reproducibility shown in 11.1.2 and 11.1.3 to judge the acceptability of resul
38、ts. NOTE Precision data were determined by a round-robin test conducted by eight laboratories using five different commercially available polyol samples covering a range of 0,3 CPR units to 1,2 CPR units. Data may be obtained from ASTM Committee D-20 or from the PURMAC committee of the American Plas
39、tics Council. 11.1.2 Repeatability (single analyst): Duplicate results obtained by the same analyst using the same equipment on the same day should only be considered suspect if they differ by more than 0,2 CPR units. This repeatability was calculated from pooled experimental data following ASTM E 1
40、80. 11.1.3 Reproducibility (multilaboratory): Results, each the mean of duplicates, obtained on identical test materials in separate laboratories should only be considered different if they differ from that of another laboratory by more than 0,6 CPR units. This reproducibility was calculated from po
41、oled experimental data following ASTM E 180. 11.2 Bias Bias is the difference between the expectation of the test results and an accepted reference value. The bias of this test has not been determined. 12 Test report The test report shall include the following: a) a reference to this International S
42、tandard; b) all details necessary to identify the product analysed; c) the results obtained, expressed as CPR units to the nearest 0,1 CPR unit, or as gKOH/g; d) any incident or detail not stipulated in this International Standard which may have influenced the result; e) the date of the analysis.ISO
43、 14899:2001(E)5 Bibliography 1 Japanese Industrial Standard K 1557:1970, Testing Method of Polyether for Polyurethane (English translation). 2 ASTM E 180, Standard Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals.BS ISO 14899:2001 BSI 389 Chiswi
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